WO2024232261A1 - 方向性電磁鋼板の製造方法 - Google Patents

方向性電磁鋼板の製造方法 Download PDF

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WO2024232261A1
WO2024232261A1 PCT/JP2024/015939 JP2024015939W WO2024232261A1 WO 2024232261 A1 WO2024232261 A1 WO 2024232261A1 JP 2024015939 W JP2024015939 W JP 2024015939W WO 2024232261 A1 WO2024232261 A1 WO 2024232261A1
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Prior art keywords
steel sheet
weight
grain
oriented electrical
annealing
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PCT/JP2024/015939
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English (en)
French (fr)
Japanese (ja)
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拓弥 山田
敬 寺島
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JFE Steel Corp
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JFE Steel Corp
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Priority to CN202480030553.3A priority Critical patent/CN121152887A/zh
Priority to KR1020257038930A priority patent/KR20250174971A/ko
Priority to JP2024550645A priority patent/JP7666756B2/ja
Priority to EP24803374.8A priority patent/EP4653557A1/en
Publication of WO2024232261A1 publication Critical patent/WO2024232261A1/ja
Anticipated expiration legal-status Critical
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    • C21D8/1255—Modifying the physical properties of ferrous metals or ferrous alloys by deformation combined with, or followed by, heat treatment during manufacturing of articles with special electromagnetic properties characterised by the heat treatment with diffusion of elements, e.g. decarburising, nitriding
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    • C21D8/00—Modifying the physical properties of ferrous metals or ferrous alloys by deformation combined with, or followed by, heat treatment
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    • C21D8/00—Modifying the physical properties of ferrous metals or ferrous alloys by deformation combined with, or followed by, heat treatment
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    • C21D8/00—Modifying the physical properties of ferrous metals or ferrous alloys by deformation combined with, or followed by, heat treatment
    • C21D8/12—Modifying the physical properties of ferrous metals or ferrous alloys by deformation combined with, or followed by, heat treatment during manufacturing of articles with special electromagnetic properties
    • C21D8/1277—Modifying the physical properties of ferrous metals or ferrous alloys by deformation combined with, or followed by, heat treatment during manufacturing of articles with special electromagnetic properties involving a particular surface treatment
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    • C21D9/00—Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor
    • C21D9/46—Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor for sheet metals
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    • C22C38/002—Ferrous alloys, e.g. steel alloys containing In, Mg, or other elements not provided for in one single group C22C38/001 - C22C38/60
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    • C22C38/18—Ferrous alloys, e.g. steel alloys containing chromium
    • C22C38/34—Ferrous alloys, e.g. steel alloys containing chromium with more than 1.5% by weight of silicon
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    • C22C38/60—Ferrous alloys, e.g. steel alloys containing lead, selenium, tellurium, or antimony, or more than 0.04% by weight of sulfur
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C22/00—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
    • C23C22/05—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions
    • C23C22/06—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous acidic solutions with pH less than 6
    • C23C22/07—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous acidic solutions with pH less than 6 containing phosphates
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    • C23C22/00—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
    • C23C22/73—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals characterised by the process
    • C23C22/74—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals characterised by the process for obtaining burned-in conversion coatings
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    • C23C22/00—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
    • C23C22/73—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals characterised by the process
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    • C23C22/00—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
    • C23C22/82—After-treatment
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
    • H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
    • H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
    • H01F1/12—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials
    • H01F1/14—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials metals or alloys
    • H01F1/147—Alloys characterised by their composition
    • H01F1/14766—Fe-Si based alloys
    • H01F1/14775—Fe-Si based alloys in the form of sheets
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
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    • H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
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    • H01F1/12—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials
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    • C21D2201/00—Treatment for obtaining particular effects
    • C21D2201/05—Grain orientation
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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Definitions

  • the present invention relates to a method for manufacturing grain-oriented electrical steel sheets with excellent coating properties over their entire length and width.
  • Grain-oriented electrical steel sheet is a soft magnetic material that is mainly used for the iron cores of transformers and the like, and is required to have excellent magnetic properties, i.e., low iron loss and high magnetic flux density.
  • Such grain-oriented electrical steel sheet is manufactured by hot rolling a material containing inhibitor-forming components such as MnS, MnSe, or AlN, annealing the hot-rolled sheet as necessary, cold rolling once or two or more times with intermediate annealing in between, decarburization annealing, applying an annealing separator mainly made of MgO to the steel sheet surface, and then finish annealing.
  • the oxide film mainly composed of SiO2 formed in the decarburization annealing reacts with the annealing separator mainly composed of MgO to form a forsterite film.
  • This forsterite film not only imparts insulation to the steel sheet surface, but also improves the magnetic properties of the steel sheet by imparting tensile stress due to its low thermal expansion.
  • a forsterite coating with excellent coating properties i.e., with high adhesion over the entire length and width of the steel sheet, is extremely important in manufacturing grain-oriented electrical steel sheet with excellent magnetic properties.
  • the decarburization annealing is a continuous annealing in a highly oxidizing atmosphere
  • the oxidizing property in the furnace is likely to vary
  • the quality of the decarburization annealed sheet is likely to vary.
  • the formation of the oxide film may also vary.
  • finish annealing is a batch annealing in coil form
  • temperature unevenness is likely to occur within the coil, which can easily lead to variations in the coating properties.
  • Patent Document 1 proposes a technology in which the annealing separator components are changed and applied in the longitudinal and transverse directions of the steel sheet.
  • Patent Document 2 proposes a technique in which light is irradiated onto the steel sheet surface and the coating adhesion is evaluated based on the brightness.
  • Patent Document 1 has problems such as high manufacturing costs, insufficient effectiveness, and still causing variation in coating characteristics.
  • Patent Document 2 had the problem that even slight differences in material components or manufacturing conditions could cause the correlation between brightness and coating adhesion to shift, making it difficult to adequately evaluate coating adhesion.
  • the present invention advantageously solves the above problems by providing a method for manufacturing grain-oriented electrical steel sheets that can stably produce grain-oriented electrical steel sheets with excellent coating properties by non-destructively grasping the coating properties over the entire length and width of the product steel sheet.
  • the gist of the present invention is as follows. 1.
  • a steel material for grain-oriented electrical steel sheet is hot-rolled, and then cold-rolled once or twice or more times with intermediate annealing in between, followed by decarburization annealing, and then an annealing separator mainly composed of MgO is applied to the surface of the steel sheet, followed by finish annealing to produce a finished sheet
  • the method includes obtaining data on the decarburization annealed sheet quality index of the steel sheet and the finish annealing conditions, and further obtaining data on the O weight and Ti+V+Zr+Nb weight contained in the forsterite coating of the finished sheet, and using the actual values of each of the weights as objective variables, and also obtaining data on the decarburization annealed sheet quality index
  • the annealing separator a prediction model for each basis weight is created by performing multiple regression analysis or machine learning using actual values of the agent composition and the finish annealing conditions as explan
  • finish annealing conditions are either or both of a H2 gas introduction temperature and a heating rate of 950 to 1100 ° C.
  • This invention makes it possible to stably manufacture grain-oriented electrical steel sheets with excellent coating properties across their entire length and width.
  • FIG. 1 is a diagram showing the Mn fluorescent X-ray intensity at each position (m, n) of a decarburized annealed sheet in a comparative example of the present invention.
  • FIG. 2 is a diagram showing the Mn intensity of fluorescent X-rays at each position (m, n) of a decarburized annealed sheet in an example of the present invention.
  • FIG. 1 is a diagram showing the temperature of the steel sheet surface when H2 gas is introduced during finish annealing at each position (m, n) in a comparative example of the present invention.
  • FIG. 1 is a diagram showing the temperature of the steel sheet surface when H2 gas is introduced during finish annealing at each position (m, n) in the inventive examples of the present invention.
  • FIG. 1 is a diagram showing the basis weight of a product sheet O at each position (m, n) in a comparative example of the present invention.
  • FIG. 1 is a diagram showing the basis weight of a product sheet O at each position (m, n) in an example of the present invention.
  • FIG. 1 is a diagram showing the product sheet (Ti+V+Zr+Nb basis weight)/O basis weight at each position (m, n) in a comparative example of the present invention.
  • FIG. 1 is a diagram showing the product sheet (Ti+V+Zr+Nb basis weight)/O basis weight at each position (m, n) in an example of the present invention.
  • the steel material composition of the grain-oriented electrical steel sheet (also simply referred to as steel sheet in this specification) in the manufacturing method of the grain-oriented electrical steel sheet according to one embodiment of the present invention will be described.
  • the steel material composition may be a conventionally known composition. Specifically, it is as follows. The balance other than the following components is Fe and unavoidable impurities. C is an effective component for improving the texture, but if the content is less than 0.01 mass%, sufficient effect cannot be obtained. On the other hand, if the content exceeds 0.1 mass%, decarburization becomes difficult and magnetic properties deteriorate. Therefore, it is preferable to set the content in the range of 0.01 to 0.1 mass%. More preferably, the lower limit is 0.02 mass% and the upper limit is 0.08 mass%.
  • Si is an effective component for increasing resistivity and improving magnetic properties, but if the content is less than 1.0 mass%, sufficient effect is not obtained. On the other hand, if the content exceeds 5.0 mass%, cold rollability deteriorates significantly. Therefore, it is preferable to set the content in the range of 1.0 to 5.0 mass%. More preferably, the lower limit is 2.0 mass% and the upper limit is 4.0 mass%.
  • Mn like Si, increases resistivity and improves magnetic properties. It is also an effective component for improving hot ductility, but if the content is less than 0.01 mass%, sufficient effect is not obtained. On the other hand, if it exceeds 0.5 mass%, the magnetic properties deteriorate. Therefore, it is preferable to set the content in the range of 0.01 to 0.5 mass%. More preferably, the lower limit is 0.02 mass% and the upper limit is 0.2 mass%.
  • MnS manganese
  • MnSe manganese
  • AlN aluminum oxide
  • the above inhibitors may be used alone or in combination.
  • one or more of the following may be added in mass percent: B: 0.0001-0.005%, Ti: 0.001-0.01%, P: 0.005-0.1%, Cr: 0.01-0.5%, Ni: 0.01-1.5%, Cu: 0.01-0.5%, Nb: 0.002-0.08%, Mo: 0.005-0.1%, Sn: 0.005-0.5%, Sb: 0.005-0.5%, and Bi: 0.001-0.05%.
  • a method for producing a grain-oriented electrical steel sheet according to an embodiment of the present invention will be described.
  • a steel material for grain-oriented electrical steel sheet adjusted to the above-mentioned chemical composition is subjected to hot rolling, and if necessary, hot-rolled sheet annealing, and then cold rolling once or two or more times with intermediate annealing therebetween, and then decarburization annealing.
  • the decarburization annealing temperature is in the range of 750 to 950°C and the time is in the range of 80 to 200 seconds. If the annealing temperature is less than 750°C and the time is less than 80 seconds, decarburization may be difficult. On the other hand, if the annealing temperature is more than 950°C and the time is more than 200 seconds, the primary recrystallized grain size will become coarse and secondary recrystallization will be suppressed, which may result in deterioration of the magnetic properties.
  • the oxidation ratio (PH 2 O/PH 2 ) of the decarburization annealing is preferably in the range of 0.3 to 0.6. If PH 2 O/PH 2 is less than 0.3, decarburization may be difficult. On the other hand, if PH 2 O/PH 2 exceeds 0.6, FeO may be formed, which may deteriorate the coating properties.
  • the decarburized annealed sheet quality index is, for example, the O concentration, Si concentration, P concentration, and Mn concentration on the steel sheet surface , the amount of SiO2 generated, the amount of FeSiO3 generated, and the amount of Fe2SiO4 generated. Furthermore, the ratio of any of these concentrations or amounts may be determined and used.
  • the decarburized annealed sheet quality index When the decarburized annealed sheet quality index is obtained by measurement, it may be measured using X-ray fluorescence analysis or infrared spectroscopy, or when it is obtained by calculation, it may be calculated from the decarburized annealing conditions such as the annealing temperature, time, and oxidation degree.
  • the steel sheet surface is coated with an annealing separator mainly composed of MgO.
  • an annealing separator mainly composed of MgO.
  • Ti, Zr, V, and Nb compounds is added to the annealing separator for the purpose of improving the coating properties.
  • the total amount of these added is preferably 1 to 7 mass% in terms of each metal element. If the amount added is less than 1 mass%, sufficient effect cannot be obtained. On the other hand, if the amount added exceeds 7 mass%, each metal element may penetrate into the steel, and the magnetic properties may deteriorate.
  • the type of compound is not limited. For example, oxides, hydroxides, borates, carbonates, nitrates, phosphates, sulfates, halides, etc. can be used. These may be used alone or in combination. It is preferable to record data on the composition of the applied annealing separator since this data will be used later when creating a prediction model.
  • oxides, hydroxides, borates, carbonates, nitrates, phosphates, sulfates, and halides of Li, Na, Mg, Al, Si, K, Ca, Fe, Co, Ni, Cu, Sr, Ba, and lanthanides may be added. These may be used alone or in combination.
  • the amount of each of these additives is preferably in the range of 0.01 to 15 parts by mass relative to 100 parts by mass of MgO. If the amount is less than 0.01 part by mass, sufficient effects cannot be obtained. On the other hand, if the amount is more than 15 parts by mass, excessive film formation or excessive suppression may occur, which may deteriorate the magnetic properties. Then, a final anneal is applied, which may include a secondary recrystallization anneal for promoting secondary recrystallization, and a purification anneal for purifying the inhibitor.
  • the annealing temperature is preferably 800 to 1000°C and the time is preferably in the range of 5 to 200 hours. If the annealing temperature is less than 800°C or the time is less than 5 hours, the secondary recrystallization may not be completed during soaking, and the magnetic properties may deteriorate. On the other hand, if the annealing temperature exceeds 1000°C or the time exceeds 200 hours, the coil may buckle and the shape may deteriorate.
  • the heating rate from 700 to 1100°C is preferably in the range of 2.5 to 50°C/h. If the heating rate is less than 2.5°C/h, the coil may buckle and the shape may deteriorate. On the other hand, if the heating rate exceeds 50°C/h, the secondary recrystallized grains may become fine and the magnetic properties may deteriorate.
  • the annealing atmosphere is an inert atmosphere of N2 or Ar.
  • the annealing temperature is 1150 to 1250°C and the time is in the range of 2 to 50 hours. If the annealing temperature is less than 1150°C or the time is less than 2 hours, there is a risk of insufficient purification. On the other hand, if the annealing temperature exceeds 1250°C or the time exceeds 50 hours, there is a risk of the coil buckling and deterioration of the shape.
  • H2 gas is introduced at any temperature in the range of 900 to 1050 ° C.
  • H2 gas By introducing H2 gas , the Fe oxide formed on the steel sheet surface is reduced, the oxidation in the furnace increases, and the formation of the coating is accelerated.
  • the H2 gas introduction temperature is less than 900 ° C, the inhibitor may decompose before the secondary recrystallization is completed, and the magnetic properties may deteriorate.
  • the H2 gas introduction temperature exceeds 1050 ° C, sufficient effect cannot be obtained.
  • data on the finish annealing conditions of the steel sheet is obtained (in this example, obtained by calculation or measurement) because it directly affects the coating properties.
  • the above-mentioned finish annealing conditions are either or both of the H2 gas introduction temperature and the heating rate between 950 and 1100 ° C.
  • the above-mentioned finish annealing conditions are obtained by measurement, they may be obtained by actual measurement with a thermocouple wound in a coil, or when they are obtained by calculation, they may be obtained by calculation from the finish annealing conditions such as the annealing temperature and time.
  • a non-destructive method for measuring the weight of each element is, for example, to measure the fluorescent X-ray intensity of each element and then convert it into the weight of each element using a calibration curve created in advance.
  • a prediction model for each basis weight is created by performing multiple regression analysis or machine learning using the actual values of each basis weight as the objective variable and the actual values of the decarburized annealed sheet quality index, the annealing separator composition, and the finish annealing conditions as explanatory variables.
  • the steel plate to be subjected to the manufacturing method of this embodiment is divided into i parts in its longitudinal direction and further divided into j parts in its width direction, and each position (m, n) (where 1 ⁇ m ⁇ i, 1 ⁇ n ⁇ j) is set.
  • the annealing separator composition and the finish annealing conditions are substituted within a certain range for the decarburization annealed sheet quality index at each of the positions (m, n), and the annealing separator composition and the finish annealing conditions are set so that the maximum O coating weight and the maximum (Ti+V+Zr+Nb coating weight)/O coating weight at each of the positions (m, n) are within a range determined by the coating adhesion.
  • each position (m, n) indicates each divided area (portion) when the steel plate is divided into i divisions in the longitudinal direction, preferably 10 to 100 divisions, and into j divisions in the width direction, preferably 5 to 20 divisions.
  • the decarburized annealed sheet quality index and the finish annealing conditions for the steel sheet are obtained (e.g., derived by calculation or measurement), and the O weight and Ti+V+Zr+Nb weight contained in the forsterite coating of the product sheet are obtained (e.g., derived by measurement), and the steel sheet may be divided into i parts in the longitudinal direction and j parts in the width direction (e.g., such calculations or measurements may be performed).
  • the formation of the coating during the final annealing may be insufficient, and the weight of O after the final annealing may be insufficient. Therefore, it is necessary to promote the formation of the coating during the final annealing and increase the weight of O by lowering the H2 gas introduction temperature during the final annealing and/or increasing the heating rate between 950°C and 1100°C.
  • Random forest or neural network may be used.
  • the fluorescent X-ray Ti intensity of the finished sheet can be measured according to the procedure described above at any point before the finishing annealing is performed and the sheet is produced.
  • the maximum range of the O basis weight is preferably 1.00 g/m2 or more . If the maximum number of the O basis weight is less than 1.00 g/ m2 , the amount of the coating formed is too small, and the coating may be easily broken by external stress, resulting in insufficient adhesion. More preferably, it is 2.00 g/m2 or more . Although there is no particular upper limit to the range of the maximum number of the O basis weight, it is preferably about 10.00 g/m2 or less because it may result in a decrease in the space factor.
  • the maximum range of the (Ti+V+Zr+Nb weight)/O weight is preferably 0.01 or more. If the value of the maximum number of (Ti+V+Zr+Nb weight)/O weight is less than 0.01, the coating adhesion may be insufficient. More preferably, it is 0.02 or more. Although the upper limit of the range of the maximum number of (Ti+V+Zr+Nb weight)/O weight is not particularly limited, it is preferably about 0.20 or less because there is a risk of each metal element penetrating into the steel.
  • the coating adhesion can be evaluated by the value of (Ti+V+Zr+Nb weight per unit area)/O weight per unit area of the product sheet is not clear, but the inventors consider it as follows. That is, the Ti, V, Zr, and Nb compounds added to the annealing separator decompose during final annealing, and are incorporated into the forsterite coating in the form of nitrides or oxides, etc., and segregate at grain boundaries, thereby increasing the strength of the coating. Therefore, it is believed that the greater the weight of Ti+V+Zr+Nb relative to the amount of the forsterite coating, the better the coating adhesion.
  • the adhesion of the forsterite coating can be evaluated by measuring the (Ti+V+Zr+Nb coating weight)/O coating weight, which allows one to estimate such grain boundary segregation.
  • the data of the decarburized annealed sheet quality index and the finish annealing conditions of the steel sheet are measured or calculated, and further, the data of the O weight and the Ti+V+Zr+Nb weight contained in the forsterite coating of the product sheet are measured.
  • the present disclosure is not limited to this case.
  • a series of data can be obtained from the outside.
  • a series of data can be obtained by a communication unit of a computer.
  • such a series of data can be obtained by a human being through transfer or the like.
  • data of the set value can be obtained instead of calculation or measurement. In this way, the acquisition of data necessary for creating a learning model can be variously modified or changed.
  • Example 1 In this example, a general machine learning tool was used to create a prediction model for each coating weight by machine learning using a neural network, with the actual values of the product sheet O coating weight and Ti+V+Zr+Nb coating weight over the past two years as the objective variables, and the actual values of the decarburized annealed sheet quality index, annealing separator composition, and finish annealing conditions as explanatory variables.
  • the sheet was then subjected to decarburization annealing in a wet hydrogen atmosphere at 840°C for 2 minutes, and then subjected to fluorescent X-ray analysis and infrared spectroscopy at each position (m, n) (where 1 ⁇ m ⁇ i, 1 ⁇ n ⁇ j) along the longitudinal direction of the steel sheet, which was divided into 50 parts (i) at a pitch of 100 m, and along the width direction of the steel sheet, which was divided into 10 parts (j) at a pitch of 100 mm, to measure the intensity of each element and the amount of each oxide generated at each position (m, n) of the steel sheet.
  • an annealing separator containing 100 parts by mass of MgO and 3 parts by mass of TiO2 was applied, and soaking treatment was performed at 850°C for 50 hours in a N2 gas atmosphere.
  • the material was then heated in the range of 950 to 1100°C at a heating rate of 15°C/h, H2 gas was introduced at a predetermined temperature, and soaking treatment was performed at 1200°C for 5 hours.
  • the final annealing was performed under the conditions of the present invention in which the H2 gas introduction temperature of the 10 coils was adjusted in the range of 900 to 1050 ° C. so that the maximum number of the product sheet O weight at each position (m, n) was 1.00 g / m2 or more and the maximum number of (Ti + V + Zr + Nb weight) / O weight was 0.01 or more, and the final annealing was performed under the conditions of the present invention in which the H2 gas introduction temperature of the 10 coils was adjusted in the range of 900 to 1050 ° C.
  • Example 2 In this example, a general machine learning tool was used to create a prediction model for each coating weight by machine learning using random forest, with the actual values of the product sheet O coating weight and Ti+V+Zr+Nb coating weight over the past two years as the objective variables, and the actual values of the decarburized annealed sheet quality index, annealing separator composition, and finish annealing conditions as explanatory variables.
  • the sheet was then decarburized and annealed in a wet hydrogen atmosphere at 840°C for 2 minutes, and then subjected to fluorescent X-ray analysis and infrared spectroscopy at each position (m, n) (where 1 ⁇ m ⁇ i, 1 ⁇ n ⁇ j) along the longitudinal direction of the steel sheet to 50 divisions (i) at a pitch of 100 m and along the width direction of the steel sheet to 10 divisions (j) at a pitch of 100 mm, to measure the intensity of each element and the amount of each oxide generated at each position (m, n) of the steel sheet.
  • an annealing separator containing 3 parts by mass of TiO2 added to 100 parts by mass of MgO was applied, and the material was heated at a heating rate of 15°C/h in the range of room temperature to 950°C, and then heated at a predetermined heating rate in the range of 950 to 1100°C.
  • H2 gas was introduced at 950°C, and the material was soaked at 1200°C for 5 hours.
  • the maximum number of the product sheet O weight at each position (m, n) was 1.00 g/m2 or more , and the maximum number of (Ti + V + Zr + Nb weight) / O weight was 0.01 or more.
  • the heating rate from 950 to 1100 ° C. was changed to 10 to 20 ° C. / h, and in each of the 10 coils, the heating rate was set to a uniform 15 ° C. / h. Finish annealing was performed. After that, a coating mainly composed of phosphate was applied, and then flattening annealing was performed at 850 ° C.
  • the percentage of positions where the maximum number of the O weight of the product sheet was 1.00 g/m2 or more and the maximum number of (Ti+V+Zr+Nb weight)/O weight was 0.01 or more was 98.7% on average for 10 coils.
  • the heating rate was set uniformly at 15° C./h, the percentage was 84.3% on average for 10 coils.

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JPH08100220A (ja) * 1994-09-30 1996-04-16 Kawasaki Steel Corp 方向性電磁鋼板の脱炭焼鈍における酸化被膜量の制御方法
JPH09184017A (ja) * 1996-01-08 1997-07-15 Kawasaki Steel Corp 高磁束密度一方向性けい素鋼板のフォルステライト被膜とその形成方法
JP2016145419A (ja) * 2015-01-30 2016-08-12 Ｊｆｅスチール株式会社 方向性電磁鋼板とその製造方法
WO2022186357A1 (ja) * 2021-03-03 2022-09-09 Ｊｆｅスチール株式会社 方向性電磁鋼板の仕上げ焼鈍条件の決定方法およびその決定方法を用いた方向性電磁鋼板の製造方法
WO2023068236A1 (ja) * 2021-10-20 2023-04-27 Ｊｆｅスチール株式会社 方向性電磁鋼板およびその製造方法

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JP5392119B2 (ja) 2010-01-29 2014-01-22 新日鐵住金株式会社 方向性電磁鋼板の酸化物被膜密着強度評価方法およびその評価装置
JP2020196773A (ja) 2019-05-30 2020-12-10 キヤノン株式会社 水性インク、インクカートリッジ、及びインクジェット記録方法

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JPS59193220A (ja) * 1983-04-15 1984-11-01 Kawasaki Steel Corp 一方向性けい素鋼板の製造方法
JPH08100220A (ja) * 1994-09-30 1996-04-16 Kawasaki Steel Corp 方向性電磁鋼板の脱炭焼鈍における酸化被膜量の制御方法
JPH09184017A (ja) * 1996-01-08 1997-07-15 Kawasaki Steel Corp 高磁束密度一方向性けい素鋼板のフォルステライト被膜とその形成方法
JP2016145419A (ja) * 2015-01-30 2016-08-12 Ｊｆｅスチール株式会社 方向性電磁鋼板とその製造方法
WO2022186357A1 (ja) * 2021-03-03 2022-09-09 Ｊｆｅスチール株式会社 方向性電磁鋼板の仕上げ焼鈍条件の決定方法およびその決定方法を用いた方向性電磁鋼板の製造方法
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